反应详情

A mixture of 4-aminopicolinic acid (2.50 g, 18.1 mmol) and conc. sulfuric acid (2 mL, 37.3 mmol) in 50 mL methanol was refluxed for 20 h. The mixture was concentrated i. vac., then 50 mL dichloromethane were added and made basic by addition of conc. ammonia (aq). Then water and NaCl (aq, sat.) were added and the aqueous layer was extracted with methylenechloride/methanol=9:1. The combined organic layers were dried over MgSO4 and then evaporated to dryness.

1. temperaturewas refluxed for 20 h
2. concentrationThe mixture was concentrated i
3. addition, then 50 mL dichloromethane were added
4. additionmade basic by addition of conc. ammonia (aq)
5. additionThen water and NaCl (aq, sat.) were added
6. extractionthe aqueous layer was extracted with methylenechloride/methanol=9:1
7. dry with materialThe combined organic layers were dried over MgSO4
8. customevaporated to dryness